Gray vat dyes and process of making.



HEINRICH BEONIATOWSKI, F BASEL, SVQ'I ZERLAND, ASSIGNOB '10 SOCIETY OFCIIEM- ICAL INDUSTRY IN BASLE, BASEL SWITZERLAND.-

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No Drawing.

To all whom it mo "concern:

Be it known that I, HEINRICH Bnoma'row- SKI, doctor of philosophy andchemist, a subject of the Emperor of Russia, and resident scribed, may

of Basel, Switzerland, have invented newand useful Gray Vat Dyestufisand a Process of Making Same, of which the following is a full, clear,and exact specification. I have founchthat valuable gray vat-dyestufisare obtained, by treating amidonaph thanthraquinone with condensingagents, as for instance antimony pentachlorid and by. subjecting theresulting product of condensati'on to the action of halogens. Theamidonaphthanthraquinone used as parent mate rial, w-hibh has hithertonowhere been debe prepared by condensing alpha-chloronaphthalene withphthalic anhydrid, transforming the resulting chloronaphthoylbenzoicacid into chloronaphthanthraquinone and substituting inthis lattef agroup amido for the chiorin atom by heating thesame with alcoholicammonia under pressure.

The process is illustrated by the following examples,

Example I: 10 parts of amid'onaphthan- 'thraquinone are boiled with 10parts of antipery reflex is isolated 'by filtration andv nitrobenzenewith mony penta 'hlorid and 100 parts of nitrobenzene for an hour in arecipient provided with a reflux cooler. The coloring matter separatedin form of small crystals of copwashed with alcohol. It dissolves in hota green-blue coloration and in concentrated sulfuric acid with anolive-brown coloration. By treating the coloring matterwit-h sodiumhydrosulfite and soda lye it yields a blue vat dyeing cotton beautifulbluish gray tints.

Example II: 10 parts "of ter obtained according to Example I are heatedto-ebullition with 100 parts nitrobenzone and 10-15 parts bromin, whilestirring, for 4 hours, in a recipient provided with a reflux cooler.After cooling of the reaction mass, the separated dyestutt is" isolatedby filtration, washed with alcohol and dried. It constitutes a bluishblack powder dissolving in-hot nitrobenzen'e-to a violet-blue solutionand in concentrated sulfuric acid to a brown solution. l'Vith all aliand hydrosulfite it Specification of Letters Patent.

\ yields a. blue vat dyeing cotton the coloring mat- Patented Aug. 30,1910.

Application filed April 4, 1910. Serial No. 553,244.

intense bluish gray tints of excellent fastness to washing, light andvchlorin.

Exampl III: 10 parts of the coloring matter prepared according toExample 1 of 66 Baum specific gravity and 8 to 10 parts bromin areallowed to flow slowl into the solution thus obtained, at a temperatureof 60 to 100 (land while stirring.

In order to finish the reaction, the mixture. s further heated forseveral hours at the specified temperature. After cooling the mass ispoured into ice water, the dyestufi' separated is isolated by filtrationand washed with water. The bluish ray paste thus obtained can beemployed directly for dyeing. The dyeings obtained on cotton show alittle .more greenish tints than those obtained with :thedyestufi ofExample II.

The brominating' can also be executed "without employment of a diluentor a solvent by direct action ofliquid bromin on the coloring matter. beaided by addition ofa halogen carrier. It is also possible-to preparethe chlorin derivatives of the coloring matter'obtained according toExample 1, the said chlorin derivatives being similar to the "describedbroniin derivatives.

"What I claim is:

1. The described process for the manufacture of gray vat-dyestufis whichconsists in treating amidonaphthanthraquinone with condensing agents andin subjecting the thus obtained coloringmatter to. the actionofhalogenating agents.

2. The described process for the manufacture of gray vat-dyestuffs,which consistsin treating amidonaphthanthraquinone 3 with are dissolvedin 200 parts 'of sulfuric acid The action of bromin can also antimony'pentachlorid and in subjecting the resulting coloring-matter totheaction of halegenating' agents.

3. The described process for the manufacture of gray vat dyestuffs whichconsists in treating amidonaphthanthraquinone with a condensing agentand in subjecting the re-- sulting coloring-matter to the action of"brominating agents.

4. The described process ture of grayvat-dyestuffs, which consists intreating amidonaphthanthraquinone with for the manufac- 10's .antimonypentachlorid and in subjecting the,

resulting coloring-matter to the action of sulfii'e :1 blue vui: dyeingmoi 011 bluish gray 10 brolnm.

i iints fast to washing", fight and chlznin. 5. As new products @110(Icscribcd 11:150- i In witness \vhm'cof l haw wrclmio signed genatedgray vat-dyestuffs derived from my mum, this 24411 day ()1 March i910,in :1midonnphthnnihraquinone, forming in dry the uv :(.-n 'c hmsubscribing wifne ses. state black powders soluble in hot nitmbcn-HEINRICH PHONEATQVFSK i.

zene with al violet-blue to blue color and in ,Vitnesms concentratedsulfurlc acld with a brown mlm' Um. Gwwnn, and ywldmg Wlth unusiac alknhand h wlw Axum Ifwrxcnj

